WO2022110455A1 - Graphene additive and preparation method therefor - Google Patents
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- WO2022110455A1 WO2022110455A1 PCT/CN2020/139974 CN2020139974W WO2022110455A1 WO 2022110455 A1 WO2022110455 A1 WO 2022110455A1 CN 2020139974 W CN2020139974 W CN 2020139974W WO 2022110455 A1 WO2022110455 A1 WO 2022110455A1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 58
- 239000000654 additive Substances 0.000 title claims abstract description 40
- 230000000996 additive effect Effects 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 238000003723 Smelting Methods 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004020 conductor Substances 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 16
- 239000011159 matrix material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 206010063401 primary progressive multiple sclerosis Diseases 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
Definitions
- the invention belongs to the technical field of additives and conductive materials, and in particular relates to a graphene additive and a preparation method.
- the present invention provides a kind of metal that can successfully add graphene to the molten state in the smelting furnace, and form multilayer graphene in the metal matrix of the prepared conductor material. , thereby greatly improving the graphene additive of the conductivity of the conductor material, and the preparation method of the graphene additive.
- the present invention adopts the following technical solutions:
- a graphene additive is made of graphene, a metal with conductivity and an organic solvent, and the volume ratios of the graphene, the metal and the organic solvent are preferably 0.28%, 14.24% and 85.48% respectively.
- the particle size of the graphene is 1-10 nm.
- the organic solvent is one of absolute ethanol, 1-3 butanediol and water, preferably absolute ethanol.
- the metal is Al or Cu.
- the present invention also provides a preparation method of the above-mentioned graphene additive, comprising the following steps:
- step a2 the mixing time in step a2 is more than 3h, and the rotating speed of the mixer is more than 2000rpm.
- step a3 the rotation speed of the centrifuge is 5000rpm, and the centrifugation time is 1h.
- the drying temperature in step a4 is 120°C
- the drying time is 24h
- the reduction temperature is 200°C
- the reduction time is 30 minutes.
- the present invention can successfully add graphene to the metal in the molten state in the smelting furnace when it is used to make the conductor material, and form multilayer graphene in the metal matrix of the prepared conductor material, thereby greatly improving the Conductivity of the conductor material.
- Fig. 1 is the schematic flow sheet of the preparation method of a kind of graphene additive of the present invention.
- the graphene additive of the present invention is made of graphene, conductive metal and organic solvent, and the volume ratio of the graphene, metal and organic solvent is preferably 0.28%, 14.24% and 85.48% respectively .
- the particle size of the graphene is 1-10 nm
- the metal can be Al or Cu
- the organic solvent is one of absolute ethanol, 1-3 butanediol, and water (preferably absolute ethanol).
- the preparation method of the graphene additive of the present invention comprises the following steps:
- Step S100 Disperse the graphene in an organic solvent to obtain a mixed solution A.
- Step S200 Add the metal into the mixed solution A, and mix to obtain the mixed solution B; specifically, use a mixer to mix the mixed solution A after adding the metal to obtain the mixed solution B, and the mixing time is preferably more than 3h, and the rotating speed of the mixer is preferably above 2000rpm.
- Step S300 Centrifuge the mixed solution B, and take off the lower layer of powder A; specifically: use a centrifuge to centrifuge the mixed solution B, and take off the lower layer of powder A, and the rotating speed of the centrifuge is preferably 5000rpm, and the centrifugation time is preferably 5000 rpm. 1h.
- Step S400 After vacuum drying the obtained lower layer powder A (for example: placing the lower layer powder A in a vacuum drying furnace for drying), charging with hydrogen at a high temperature for reduction to obtain powder B; wherein the drying temperature is preferably 120°C, The drying time is preferably 24h, the reduction temperature is preferably 200°C, and the reduction time is preferably 30 minutes.
- the drying temperature is preferably 120°C
- the drying time is preferably 24h
- the reduction temperature is preferably 200°C
- the reduction time is preferably 30 minutes.
- Step S500 Add a smelting additive (such as a refiner, the smelting additive is completely volatilized during the grinding process) into the powder B, and grind to obtain the powder C;
- a smelting additive such as a refiner, the smelting additive is completely volatilized during the grinding process
- Step S600 Press the powder C to obtain a graphene additive.
- the graphene additive of the present invention When the graphene additive of the present invention is used to make the conductor material, the graphene can be successfully added to the metal in the molten state in the smelting furnace, and the multi-layer graphene is formed in the metal matrix of the prepared conductor material, Thereby, the conductivity of the conductor material is greatly improved.
- the present embodiment 1 is made of graphene, Cu powder and dehydrated alcohol as a graphene additive, and the specific steps are:
- the graphene additive obtained in Example 1 and Al are made into conductor materials, and the specific preparation process is as follows: at first, Al is put into a smelting furnace and melted; then the graphene additive is added into the smelting furnace, mixed with molten Al, and finally stirred. , and heat preservation for 1 h to obtain a conductive material.
- the present embodiment 2 is made of graphene, Cu powder and dehydrated alcohol to make graphene additive, and the concrete steps are:
- the graphene additive obtained in Example 2 and Cu are made into conductor materials, and the specific preparation process is as follows: at first Cu is put into a smelting furnace and melted; then the graphene additive is added into the smelting furnace, mixed with molten Cu, and finally stirred. , and heat preservation for 1 h to obtain a conductive material.
- test Examples 1-2 and conventional aluminum sheets were entrusted to test Examples 1-2 and conventional aluminum sheets as a comparative example, specifically: by using American Quantum PPMS-9 testing equipment to test, test items and conditions: resistivity (300K), test results Table 1 below.
Abstract
The present invention relates to a graphene additive and a preparation method therefor. The graphene additive is prepared from graphene, a conductive metal and an organic solvent, and the volume ratio of the graphene, the metal and the organic solvent is preferably 0.28%, 14.24% and 85.48%, respectively. By using the graphene additive for manufacturing a conductor material, graphene can be successfully added to a molten metal in a smelting furnace, and multiple layers of graphene are formed in the metal matrix of the manufactured conductor material, thereby improving the conductivity of the conductor material.
Description
本发明属于添加剂和导电材料技术领域，具体涉及一种石墨烯添加剂及制备方法。The invention belongs to the technical field of additives and conductive materials, and in particular relates to a graphene additive and a preparation method.
目前，常用的导电材料有银、铜、金、铝、钨、镍、铁、铅等。但是，申请人发现：现有的这些导电材料的电阻率较高，从而使导电率偏低，自身耗能较高，发热量大，使用寿命大大缩短。At present, commonly used conductive materials are silver, copper, gold, aluminum, tungsten, nickel, iron, lead, etc. However, the applicant found that these existing conductive materials have high resistivity, so that the electrical conductivity is low, the energy consumption is high, the calorific value is large, and the service life is greatly shortened.
发明内容SUMMARY OF THE INVENTION
为解决现有技术中存在的上述问题，本发明提供了一种能够成功将石墨烯加入到熔炼炉内的熔化状态的金属中，并在制成的导体材料的金属基体内形成多层石墨烯，从而大大提升导体材料导电率的石墨烯添加剂，以及该石墨烯添加剂的制备方法。In order to solve the above-mentioned problems existing in the prior art, the present invention provides a kind of metal that can successfully add graphene to the molten state in the smelting furnace, and form multilayer graphene in the metal matrix of the prepared conductor material. , thereby greatly improving the graphene additive of the conductivity of the conductor material, and the preparation method of the graphene additive.
为解决上述技术问题，本发明采用如下技术方案：In order to solve the above-mentioned technical problems, the present invention adopts the following technical solutions:
一种石墨烯添加剂，由石墨烯、具有导电性的金属和有机溶剂制成，且所述石墨烯、金属和有机溶剂的体积比分别优选为0.28％、14.24％和85.48％。A graphene additive is made of graphene, a metal with conductivity and an organic solvent, and the volume ratios of the graphene, the metal and the organic solvent are preferably 0.28%, 14.24% and 85.48% respectively.
进一步地，所述石墨烯的粒径为1～10nm。Further, the particle size of the graphene is 1-10 nm.
进一步地，所述有机溶剂是无水乙醇、1-3丁二醇、水中的一种，优选无水乙醇。Further, the organic solvent is one of absolute ethanol, 1-3 butanediol and water, preferably absolute ethanol.
进一步地，所述金属是Al或Cu。Further, the metal is Al or Cu.
本发明还提供了一种上述石墨烯添加剂的制备方法，包括以下步骤：The present invention also provides a preparation method of the above-mentioned graphene additive, comprising the following steps:
a1.将石墨烯分散于有机溶剂，得到混合溶液A；a1. Graphene is dispersed in an organic solvent to obtain mixed solution A;
a2.将金属加入混合溶液A中，混合得到混合溶液B；a2. Add the metal into the mixed solution A, and mix to obtain the mixed solution B;
a3.对混合溶液B进行离心处理，并取下层粉末A；a3. Centrifuge the mixed solution B, and remove the lower layer of powder A;
a4.对取得的下层粉末A进行真空干燥后，在高温下充入氢气还原，得到粉末B；a4. After vacuum-drying the obtained lower layer powder A, fill it with hydrogen at a high temperature for reduction to obtain powder B;
a5.在粉末B中加入熔炼添加剂进行研磨，得到粉末C；a5. Add smelting additives to powder B for grinding to obtain powder C;
a6.将粉末C压制成型，得到石墨烯添加剂。a6. Press the powder C to obtain the graphene additive.
进一步地，步骤a2中的混合时间在3h以上，混合器的转速在2000rpm以上。Further, the mixing time in step a2 is more than 3h, and the rotating speed of the mixer is more than 2000rpm.
进一步地，步骤a3中离心机的转速为5000rpm，离心时间为1h。Further, in step a3, the rotation speed of the centrifuge is 5000rpm, and the centrifugation time is 1h.
进一步地，步骤a4中的干燥温度为120℃，干燥时间为24h，还原温度为200℃，还原时间为30分钟。Further, the drying temperature in step a4 is 120°C, the drying time is 24h, the reduction temperature is 200°C, and the reduction time is 30 minutes.
本发明主要具有以下有益效果：The present invention mainly has the following beneficial effects:
本发明通过上述技术方案，即可用于制作导体材料时成功将石墨烯加入到熔炼炉内的熔化状态的金属中，并在制成的导体材料的金属基体内形成多层石墨烯，从而大大提升导体材料的导电率。Through the above technical solutions, the present invention can successfully add graphene to the metal in the molten state in the smelting furnace when it is used to make the conductor material, and form multilayer graphene in the metal matrix of the prepared conductor material, thereby greatly improving the Conductivity of the conductor material.
图1是本发明所述的一种石墨烯添加剂的制备方法的流程示意图。Fig. 1 is the schematic flow sheet of the preparation method of a kind of graphene additive of the present invention.
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention.
本发明所述的一种石墨烯添加剂，由石墨烯、具有导电性的金属 和有机溶剂制成，且所述石墨烯、金属和有机溶剂的体积比分别优选为0.28％、14.24％和85.48％。所述石墨烯的粒径为1～10nm，所述金属可以是Al或Cu，所述有机溶剂是无水乙醇、1-3丁二醇、水中的一种(优选无水乙醇)。The graphene additive of the present invention is made of graphene, conductive metal and organic solvent, and the volume ratio of the graphene, metal and organic solvent is preferably 0.28%, 14.24% and 85.48% respectively . The particle size of the graphene is 1-10 nm, the metal can be Al or Cu, and the organic solvent is one of absolute ethanol, 1-3 butanediol, and water (preferably absolute ethanol).
如图1所示，本发明所述石墨烯添加剂的制备方法，包括以下步骤：As shown in Figure 1, the preparation method of the graphene additive of the present invention comprises the following steps:
步骤S100.将石墨烯分散于有机溶剂，得到混合溶液A。Step S100. Disperse the graphene in an organic solvent to obtain a mixed solution A.
步骤S200.将金属加入混合溶液A中，混合得到混合溶液B；具体为采用混合器对加入金属后混合溶液A进行混合，得到混合溶液B，而且混合时间优选在3h以上，混合器的转速优选在2000rpm以上。Step S200. Add the metal into the mixed solution A, and mix to obtain the mixed solution B; specifically, use a mixer to mix the mixed solution A after adding the metal to obtain the mixed solution B, and the mixing time is preferably more than 3h, and the rotating speed of the mixer is preferably above 2000rpm.
步骤S300.对混合溶液B进行离心处理，并取下层粉末A；具体为：利用离心机对混合溶液B进行离心处理，并取下层粉末A，而且离心机的转速优选为5000rpm，离心时间优选为1h。Step S300. Centrifuge the mixed solution B, and take off the lower layer of powder A; specifically: use a centrifuge to centrifuge the mixed solution B, and take off the lower layer of powder A, and the rotating speed of the centrifuge is preferably 5000rpm, and the centrifugation time is preferably 5000 rpm. 1h.
步骤S400.对取得的下层粉末A进行真空干燥后(比如：将下层粉末A放入真空干燥炉中进行干燥)，在高温下充入氢气还原，得到粉末B；其中干燥温度优选为120℃，干燥时间优选为24h，还原温度优选为200℃，还原时间优选为30分钟。Step S400. After vacuum drying the obtained lower layer powder A (for example: placing the lower layer powder A in a vacuum drying furnace for drying), charging with hydrogen at a high temperature for reduction to obtain powder B; wherein the drying temperature is preferably 120°C, The drying time is preferably 24h, the reduction temperature is preferably 200°C, and the reduction time is preferably 30 minutes.
步骤S500.在粉末B中加入熔炼添加剂(如：细化剂，该熔炼添加剂在研磨过程全部挥发。)进行研磨，得到粉末C；Step S500. Add a smelting additive (such as a refiner, the smelting additive is completely volatilized during the grinding process) into the powder B, and grind to obtain the powder C;
步骤S600.将粉末C压制成型，得到石墨烯添加剂。Step S600. Press the powder C to obtain a graphene additive.
将本发明所述石墨烯添加剂用于制作导体材料时，即可成功将石墨烯加入到熔炼炉内的熔化状态的金属中，并在制成的导体材料的金属基体内形成多层石墨烯，从而大大提升了导体材料的导电率。When the graphene additive of the present invention is used to make the conductor material, the graphene can be successfully added to the metal in the molten state in the smelting furnace, and the multi-layer graphene is formed in the metal matrix of the prepared conductor material, Thereby, the conductivity of the conductor material is greatly improved.
下面通过具体实施例进一步对本发明所述石墨烯添加剂及制备 方法做进一步说明。Graphene additive of the present invention and preparation method are further described below by specific embodiment.
实施例1：
Example 1 :
本实施例1由石墨烯、Cu粉末和无水乙醇制成石墨烯添加剂，具体步骤为：The present embodiment 1 is made of graphene, Cu powder and dehydrated alcohol as a graphene additive, and the specific steps are:
1)将适量的石墨烯添加剂分散于无水乙醇，得到混合溶液A；1) Disperse an appropriate amount of graphene additive in absolute ethanol to obtain mixed solution A;
2)将50g的Cu粉末加入混合溶液A中，并采用混合器以2000rpm以上的转速混合3h以上，得到混合溶液B；2) adding 50 g of Cu powder into mixed solution A, and using a mixer to mix at a speed of more than 2000 rpm for more than 3 h to obtain mixed solution B;
3)利用离心机在5000rpm的转速下对混合溶液B进行离心处理1h，并取下层粉末A；3) Centrifuge the mixed solution B for 1 h at a rotating speed of 5000 rpm using a centrifuge, and remove the lower layer of powder A;
4)对取得的下层粉末A放入真空干燥炉内，并在120℃下进行真空干燥24h，然后在200℃的高温下充入氢气还原30分钟，得到粉末B；4) Put the obtained lower layer powder A into a vacuum drying furnace, and vacuum-dry it at 120°C for 24 hours, and then charge it with hydrogen at a high temperature of 200°C for 30 minutes to reduce to obtain powder B;
5)在粉末B中加入熔炼添加剂进行研磨，得到粉末C；5) adding smelting additives in powder B and grinding to obtain powder C;
6)将粉末C压制成型，得到石墨烯添加剂。6) Pressing the powder C to obtain the graphene additive.
将实施例1制得的石墨烯添加剂与Al制成导体材料，具体制备过程为：首先将Al放入熔炼炉进行熔化；接着将石墨烯添加剂加入熔炼炉中，与熔化的Al混合，最后搅拌、保温1h，制得导电材料。The graphene additive obtained in Example 1 and Al are made into conductor materials, and the specific preparation process is as follows: at first, Al is put into a smelting furnace and melted; then the graphene additive is added into the smelting furnace, mixed with molten Al, and finally stirred. , and heat preservation for 1 h to obtain a conductive material.
实施例2：
Example 2 :
本实施例2由石墨烯、Cu粉末和无水乙醇制成石墨烯添加剂，具体步骤为：The present embodiment 2 is made of graphene, Cu powder and dehydrated alcohol to make graphene additive, and the concrete steps are:
1)将适量的石墨烯添加剂分散于无水乙醇，得到混合溶液A；1) Disperse an appropriate amount of graphene additive in absolute ethanol to obtain mixed solution A;
2)将50g的Cu粉末加入混合溶液A中，并采用混合器以2000rpm以上的转速混合3h以上，得到混合溶液B；2) adding 50 g of Cu powder into mixed solution A, and using a mixer to mix at a speed of more than 2000 rpm for more than 3 h to obtain mixed solution B;
3)利用离心机在5000rpm的转速下对混合溶液B进行离心处理 1h，并取下层粉末A；3) using a centrifuge to perform centrifugation on mixed solution B for 1 h at a rotating speed of 5000 rpm, and remove the lower layer of powder A;
4)对取得的下层粉末A放入真空干燥炉内，并在120℃下进行真空干燥24h，然后在200℃的高温下充入氢气还原30分钟，得到粉末B；4) Put the obtained lower layer powder A into a vacuum drying furnace, and vacuum-dry it at 120°C for 24 hours, and then charge it with hydrogen at a high temperature of 200°C for 30 minutes to reduce to obtain powder B;
5)在粉末B中加入熔炼添加剂进行研磨，得到粉末C；5) adding smelting additives in powder B and grinding to obtain powder C;
6)将粉末C压制成型，得到石墨烯添加剂。6) Pressing the powder C to obtain the graphene additive.
将实施例2制得的石墨烯添加剂与Cu制成导体材料，具体制备过程为：首先将Cu放入熔炼炉进行熔化；接着将石墨烯添加剂加入熔炼炉中，与熔化的Cu混合，最后搅拌、保温1h，制得导电材料。The graphene additive obtained in Example 2 and Cu are made into conductor materials, and the specific preparation process is as follows: at first Cu is put into a smelting furnace and melted; then the graphene additive is added into the smelting furnace, mixed with molten Cu, and finally stirred. , and heat preservation for 1 h to obtain a conductive material.
经委托华南理工大学材料学院对实施例1-2以及常规铝片作为对比例进行检测，具体为：通过采用美国量子PPMS-9检测设备检测，检测项目和条件：电阻率(300K)，检测结果如下表1。The School of Materials, South China University of Technology was entrusted to test Examples 1-2 and conventional aluminum sheets as a comparative example, specifically: by using American Quantum PPMS-9 testing equipment to test, test items and conditions: resistivity (300K), test results Table 1 below.
表1Table 1
从上表可以看出，将本发明的石墨烯添加剂用于制做实施例1-2的导体材料，即可在Al基体和Cu基体内形成多层石墨烯，从而使导体材料与常规的铝片相比，电阻率明显减小，导电率大大提升。It can be seen from the above table that when the graphene additive of the present invention is used to make the conductor material of Example 1-2, multilayer graphene can be formed in the Al matrix and the Cu matrix, so that the conductor material can be compared with the conventional aluminum matrix. Compared with the sheet, the resistivity is significantly reduced, and the conductivity is greatly improved.
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也视为本发明的保护范围。The above are the preferred embodiments of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications can also be made, and these improvements and modifications may also be regarded as It is the protection scope of the present invention.
Claims (8)
- 一种石墨烯添加剂，其特征在于，由石墨烯、具有导电性的金属和有机溶剂制成，且所述石墨烯、金属和有机溶剂的体积比分别优选为0.28％、14.24％和85.48％。A graphene additive is characterized in that, it is made of graphene, conductive metal and organic solvent, and the volume ratio of the graphene, metal and organic solvent is preferably 0.28%, 14.24% and 85.48% respectively.
- 根据权利要求1所述的石墨烯添加剂，其特征在于，所述石墨烯的粒径为1～10nm。The graphene additive according to claim 1, wherein the graphene has a particle size of 1-10 nm.
- 根据权利要求1所述的石墨烯添加剂，其特征在于，所述有机溶剂是无水乙醇、1-3丁二醇、水中的一种，优选无水乙醇。Graphene additive according to claim 1, is characterized in that, described organic solvent is a kind of dehydrated alcohol, 1-3 butanediol, water, preferably dehydrated alcohol.
- 根据权利要求1所述的石墨烯添加剂，其特征在于，所述金属是Al或Cu。The graphene additive according to claim 1, wherein the metal is Al or Cu.
- 一种权利要求1-4中任一所述的石墨烯添加剂的制备方法，其特征在于，包括以下步骤：A preparation method of the graphene additive described in any one of the claims 1-4, is characterized in that, comprises the following steps:a1.将石墨烯分散于有机溶剂，得到混合溶液A；a1. Graphene is dispersed in an organic solvent to obtain mixed solution A;a2.将金属加入混合溶液A中，混合得到混合溶液B；a2. Add the metal into the mixed solution A, and mix to obtain the mixed solution B;a3.对混合溶液B进行离心处理，并取下层粉末A；a3. Centrifuge the mixed solution B, and remove the lower layer of powder A;a4.对取得的下层粉末A进行真空干燥后，在高温下充入氢气还原，得到粉末B；a4. After vacuum-drying the obtained lower layer powder A, fill it with hydrogen at a high temperature for reduction to obtain powder B;a5.在粉末B中加入熔炼添加剂进行研磨，得到粉末C；a5. Add smelting additives to powder B for grinding to obtain powder C;a6.将粉末C压制成型，得到石墨烯添加剂。a6. Press the powder C to obtain the graphene additive.
- 根据权利要求5所述的制备方法，其特征在于，步骤a2中的混合时间在3h以上，混合器的转速在2000rpm以上。The preparation method according to claim 5, wherein the mixing time in step a2 is more than 3h, and the rotating speed of the mixer is more than 2000rpm.
- 根据权利要求5所述的制备方法，其特征在于，步骤a3中离心机的转速为5000rpm，离心时间为1h。The preparation method according to claim 5, wherein in step a3, the rotating speed of the centrifuge is 5000rpm, and the centrifugation time is 1h.
- 根据权利要求5所述的制备方法，其特征在于，步骤a4中的干燥温度为120℃，干燥时间为24h，还原温度为200℃，还原时间为30分钟。The preparation method according to claim 5, wherein the drying temperature in step a4 is 120°C, the drying time is 24h, the reduction temperature is 200°C, and the reduction time is 30 minutes.
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